LC-MS/MS鉴别地沟油新方法

A Novel Method for the Identification of Gutter Oils Using LC-MS/MS

建立了高效液相色谱-串联质谱(LC-MS/MS)同时测定地沟油中辣椒素、二氢辣椒素及胡椒碱3种难挥发性微量杂质成分的方法。样品采用正己烷饱和的乙腈提取,经Thermo BDS Hypersil C18(100 mm×2.1 mm,2.4μm)色谱柱梯度洗脱分离,在电喷雾正离子模式下以多反应监测(MRM)方式采集数据进行定性定量测定。3种地沟油特征物质在相应的浓度范围内呈良好线性,相关系数(r2)均大于0.99,在3个不同加标水平下,平均回收率为65%～89%,相对标准偏差(RSD)为5.3%～16.1%,检出限(LOD,S/N≥3)和定量下限(LOQ,S/N≥10)分别为0.03、0.1μg/kg。实际样品测试表明,该方法简便快速、灵敏可靠,可作为地沟油鉴别的重要手段之一。

A novel method was developed for the simultaneous determination of three trace non-volatile impurities,capsaicin,dihydrocapsaicin and piperine in gutter oils using liquid chromatography-tandem mass spectrometry（LC-MS/MS）.Analytes were extracted with hexane saturated acetonitrile,then separated on a Thermo BDS Hypersil C18 column（100 mm×2.1 mm,2.4 μm）by gradient elution.The qualitative and quantitative analysis of target compounds were carried out by electrospray ionization mass spectrometry under the positive mode with multiple reaction monitoring（MRM）.The correlation coefficients of three calibration curves were over 0.99 in the corresponding concentration range.The average recoveries of three analytes varied from 65% to 89%,with relative standard deviations（RSDs） of 5.3%-16.1%.The limits of detection（LOD,S/N≥3） and quantitation（LOQ,S/N≥10） were 0.03 μg/kg and 0.1 μg/kg,respectively.The results of the real sample tests showed that this method is simple,rapid,sensitive and reliable,and could be used as one of the identification means for gutter oils.